Triethylamine → Coumate

HRID 327705

반응식

HRID 327705 반응식
[OH:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6]([CH3:13])=[CH:7][C:8](=[O:12])[O:9]2)=[CH:4][CH:3]=1.[S:14](Cl)(=[O:17])(=[O:16])[NH2:15].C(N(CC)CC)C>C(#N)C>[CH3:13][C:6]1[C:5]2[CH:4]=[CH:3][C:2]([O:1][S:14](=[O:17])(=[O:16])[NH2:15])=[CH:11][C:10]=2[O:9][C:8](=[O:12])[CH:7]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 24499Chlorosulfamic acidHCID 52805674-Methylumbelliferone

생성물 1

HCID 9859866Coumate수율 41.1%

시약·촉매·용매 1

HCID 6342Acetonitrile용매2회

실험 절차

A slurry of 7-hydroxy-4-methylcoumarin (17.6 g, 0.10 mole) in acetonitrile (100 ml) was treated with a total of 84 ml of 3M sulfamoyl chloride (0.255 mole) in acetonitrile. The mixture was then treated dropwise with triethylamine (25.8 g, 0.255 mole). The reaction temperature was allowed to rise to 45° without any cooling. The mixture was stirred overnight at ambient temperature. The precipitate was collected, triturated with water, and dried in a vacuum oven at 70° C. for 15 hr to give 10.5 g (41%) of white powder, mp 161°-164° C.

후처리

  1. customto rise to 45° without any cooling
  2. customThe precipitate was collected
  3. customtriturated with water
  4. customdried in a vacuum oven at 70° C. for 15 hr

출처 및 근거

ORD 기록
ord-716ec8270da347688c7babe111970277
출처 데이터셋
uspto-grants-1993_12
특허 번호
US05273993

연결된 노트

불러오는 중…